Quantitative determination of 58 aromatic amines and positional isomers in textiles by high-performance liquid chromatography with electrospray ionization tandem mass spectrometry
Quantitative determination of 58 aromatic amines and positional isomers in textiles by high-performance liquid chromatography with electrospray ionization tandem mass spectrometry
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DOI：
10.1016/j.chroma.2019.01.039
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发表时间：
2019-05-10
影响因子：
4.1
通讯作者：
Deflorin, Otmar
中科院分区：
文献类型：
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作者：
Kaempfer, Patrick;Crettaz, Stephanie;Deflorin, Otmar
描述了一种同时测定服装纺织品中 58 种芳香胺 (AA) 的简单方法。在测试的胺中，有 22 种已知致癌物并受欧洲法律监管。预计纺织品中还会出现其他不受管制的胺，这些胺被怀疑具有致癌性或致突变性。本研究的重点是获得一种具有受监管和不受监管的氨基酸的多方法，并分离特定胺的不同位置异构体。为了实现这一目标，对柱相化学和流动相 pH 等 HPLC 参数进行了优化。所有其他胺均采用与位置异构体评估相同的条件进行分离。根据 DIN EN 14362-1，样品制备被减少到最低限度。对提取物进行还原裂解和稀释后，制备样品用于 LC-MS/MS 分析。使用这种改进的样品制备方法，不再需要用硅藻土进一步净化样品。通过向空白纺织品的提取物中添加所选的胺来验证该方法。定量下限 (LLOQ) 范围为 1 至 10 mg kg(-1)。获得了从 10 到 500 mu g L-1 的出色线性度，系数 (r) 高于 0.99，允许对样品强制通过零进行单点校准（300 mu g L-1 对应于纺织品中的 60 mg kg(-1)）。回收率范围为 88% 至 116%，日内和日间精度值为 1.8-12.1%。该方法的准确性经过认证标准物质（iis18A03，荷兰实验室研究所）的测试，显示出高于95%的出色回收率。最终，该方法成功应用于150个不同纺织纤维和颜色的真实样品。通过光谱库和离子比率确认了阳性结果。 (C) 2019 Elsevier B.V. 保留所有权利。
A straightforward method for simultaneous determination of 58 aromatic amines (AAs) in clothing textiles is described. Of the tested amines, 22 are known carcinogens and regulated under European law. Further unregulated amines, which are suspected to be carcinogenic or mutagenic, are also expected to occur in textiles. The focus of this study was to obtain a multimethod with regulated and unregulated AAs and to separate different positional isomers of specific amines. To achieve this goal, the HPLC parameters such as column phase chemistry and mobile phase pH were optimized. All other amines were separated with the same conditions evaluated for the positional isomers. The sample preparation was reduced to a minimum in accordance to DIN EN 14362-1. After reductive cleavage and dilution of the extracts, the samples were prepared for LC-MS/MS analysis. Further cleanup of the samples with diatomaceous earth was no longer required with this modified sample preparation.The method was validated by spiking the extracts of blank textiles with the chosen amines. Lower Limits of Quantification (LLOQs) ranged from 1 to 10 mg kg(-1). Excellent linearity from 10 to 500 mu g L-1 was obtained with coefficients (r) higher than 0.99 allowing a one-point calibration (300 mu g L-1 corresponding to 60 mg kg(-1) in textiles) forced through zero for the samples. Recovery ranged from 88 to 116% with intra- and inter-day precision values of 1.8-12.1%. The accuracy of this method was tested by a certified reference material (iis18A03, Institute for laboratory Studies, the Netherlands) and showed excellent recoveries higher than 95%.Finally, the described method was successfully applied on 150 real samples with different textile fibres and colours. Positive results were confirmed by means of the spectral library and with the ion ratios. (C) 2019 Elsevier B.V. All rights reserved.